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Ethanethiol → HCID 13210512, Verbindung

HRID 1462238
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1462238
[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([N:21]([CH2:28]OC(=O)C(C)(C)C)[C:22]3[N:27]=[CH:26][CH:25]=[CH:24][N:23]=3)=[CH:17][CH:16]=2)[C:10](=[O:36])[C:9]1=[O:37])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.O1CCOCC1.[CH2:45]([SH:47])[CH3:46]>>[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][C:15]2[CH:16]=[CH:17][C:18]([N:21]([CH2:28][S:47][CH2:45][CH3:46])[C:22]3[N:27]=[CH:26][CH:25]=[CH:24][N:23]=3)=[CH:19][CH:20]=2)[C:10](=[O:36])[C:9]1=[O:37])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 6343EthanethiolHCID 13210503HCID 13210503, VerbindungHCID 204431481,4-Dioxane hydrochloride

Produkt 1

HCID 13210512HCID 13210512, VerbindungAusbeute 86,8 %

Versuchsvorschrift

In 10 ml of ethyl mercaptan was dissolved 1.0 g of 1-benzyl-4-{4-[N-pivaloyloxymethyl-N-(2-pyrimidinyl)amino]benzyl}-2,3-dioxopiperazine, and 0.01 ml of 5.7 N hydrogen chloride-dioxane solution was added thereto, after which the resulting mixture was subjected to reaction at room temperature for 3 hours. After the completion of the reaction, the reaction mixture was distilled under reduced pressure, and 50 ml of diisopropyl ether was added to the crystals thus obtained, after which the resulting crystals were filtered. The crystals thus obtained were recrystallized from isopropyl alcohol to obtain 0.8 g (86.8% yield) of white crystalline 1-benzyl-4-{4-[N-ethylthiomethyl-N-(2-pyrimidinyl)amino]benzyl}-2,3-dioxopiperazine having a melting point of 144° C.

Aufarbeitung

  1. additionwas added
  2. customafter which the resulting mixture was subjected to reaction at room temperature for 3 hours
  3. customAfter the completion of the reaction
  4. distillationthe reaction mixture was distilled under reduced pressure, and 50 ml of diisopropyl ether
  5. additionwas added to the crystals
  6. customthus obtained
  7. filtrationafter which the resulting crystals were filtered
  8. customThe crystals thus obtained
  9. customwere recrystallized from isopropyl alcohol

Quellen und Nachweise

ORD-Eintrag
ord-3c33942e5a684f19b44bd505e08dcda9
Quelldatensatz
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04459407

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